Determination of trace 2,4-dichlorophenoxyacetic acid in fresh produce by gas chromatography with boron trichloride/2-chloroethanol derivatization.
2,4-Dichlorophenoxyacetic acid (2,4-D) residues in fresh produce is officially analyzed as its methyl ester form by gas chromatography with electron capture detection (GC-ECD). Because of safety concerns with diazomethane, the reagent used to form methyl esters, a less toxic and dangerous reagent, BCl3/2-chloroethanol, was considered. With this alternative reagent, the detecting product is a 2-chloroethyl ester. Compared with the methylester, the 2-chloroethylester has a longer retention time and a better signal-to-noise ratio for trace level analysis by GC-ECD. However, the reagent produces too many unwanted background peaks. If peak retention time is the only information available to identify the residue in case of litigation, the presence of too much background noise increases the ambiguity of identification. Therefore, confirmation by interpretation of the mass spectrum and determination of the compound structure is necessary to ensure the validity of the method. Ten commodities were fortified with 2,4-D at 0.1 ppm. Recoveries of 2-chloroethyl esters and methyl esters were 91 and 92%, respectively. The method is safe, simple, and robust.
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State of California, Department of Food and Agriculture, Anaheim, CA 92801, USA.
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D015084:2,4-Dichlorophenoxyacetic Acid / Q000032:analysis*; D001880:Boranes; D002712:Chlorides; D002849:Chromatography, Gas; D005023:Ethylene Chlorohydrin; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D006540:Herbicides / Q000032:analysis*; D010573:Pesticide Residues / Q000032:analysis*; D014675:Vegetables / Q000737:chemistry*
D001880:Boranes; D002712:Chlorides; D006540:Herbicides; D010573:Pesticide Residues; D015084:2,4-Dichlorophenoxyacetic Acid; D005023:Ethylene Chlorohydrin; C092267:boron trichloride